This document describes a procedure for determining the amount of sulfate in an unknown sample using gravimetric analysis with barium sulfate precipitation. Key steps include: 1) Adding barium chloride to the sample to precipitate out barium sulfate; 2) Filtering and drying the barium sulfate precipitate; 3) Weighing the precipitate and calculating the sulfate concentration based on the precipitate mass. The procedure aims to quantify sulfate using a precipitation gravimetry technique. Results indicated a sulfate concentration of 4.342 mg/L in the unknown sample.

1. KWAME NKRUMAH UNIVERSITY OF SCIENCE AND
TECHNOLOGY, KUMASI
COLLEGE OF SCIENCE
DEPARTMENT OF CHEMISTRY
PRATICAL CHEMISTRY IV
ANALYTICAL PRACTIAL 2.2.2
NAME: ADU AUGUSTINE
DATE: 3RD FEBRUARY, 2014.

2. DETERMINATION OF SULPHATE AS BARIUMSULPHATE USING
GRAVIMETRY WITH DRYING OF RESIDUE
AIMS AND OBJECTIVES:
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To determine the amount of sulphate in an unknown sulfate sample
To perform and develop skills in precipitation Gravimetric method of qualitative analysis.
INTRODUCTION
Gravimetric includes all analytical methods in which the analytical signal is a measurement of
mass or change in mass. There are four types of gravimetric method:
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Precipitation gravimetry
Electrogravimetry
Volatilization gravimetry
Particular gravimetry
In precipitation gravimetry an insoluble compound forms when we add a precipitating reagent or
precipitant to a solution containing the analyte. In most methods the precipitate is the product of
a simple metathesis reaction between the analyte and precipitant, however, any reaction
generating a precipitate can potentially serve as gravimetric method.
All precipitation gravimetric analysis share two attributes. Firstly, the precipitate must be of low
solubility, of high purity and of known composition if its mass is to accurately reflect the
analyte`s mass. Secondly, the precipitate must be separate from the reaction mixture. To provide
accurate result, solubility must minimal.
Sulphate is widely distributed in nature and may be present in natural water in concentration
ranging from a few to several thousand milligram/liter. Sulphates are of considerable concern
because they are indirectly responsible for two serious problems often associated with the
handling and treatment of water. Odour and sewer corrosion problem result from the reduction of
sulphate hydrogen sulphide under anaerobic conditions.
Sulphate can be determined by
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Gravimetric method of with ignition of residue
Gravimetric method with drying of residue
Turbidimetric method
Gravimetric method with ignition of residue
Sulphate is precipitated in hydrochloric acid medium as barium sulphate by the addition of
barium chloride. The precipitation is carried out near the boiling point temperature and after a
period of digestion, the precipitate is filtered, washed with water until free of chloride, ignited
weighed barium sulphate.

3. Gravimetric method with drying of residue
If organic matter is not present in the sample first method can be done without igniting and
instead drying the residue and weighing.
Turbidimetric method
Turbidimetric method is method of measuring sulphate is based upon the fact that barium
sulphate tends to precipitate in a colloidal form and that this tendency is enchance in presence of
sodium chloride – hydrochloric acid solution containing glycerol and other organic compounds.
The absorbance of barium sulphate solution is measured by nephelometer or turbidmeter and the
sulphate ion concentration determined by the comparison of the reading with a standard curve.
SOLUTION AND CHEMICAL
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1+1 HCl
0.05M BaCL2
0.1M HNO3
AgNO3
Unknown sample
Warm water
APPARATUS
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400ml beaker
10ml and 200ml measuring cylinder
Stirring rod
Heating plate
Desicator
Analytical balance
Filter paper
Vacuum pump compressor
PROCEDURE
250ml of the unknown sample is measured and put into 400ml beaker. Addition of 3ml 1+1HCl
is poured into the 400ml beaker containing the unknown sample.
The solution is heated to near boiling point and slowly 80ml of 0.05M BaCl2 is added with
efficient stirring.
The mixture solution is left to digest for about 30minutes near boiling point. Afterward the
solution is allowed to settle for the precipitate to form at the basement. A few drops of BaCl2 is
added to the clear solution at the top of the precipitate check all the sulphate in the solution is
precipitated out. If not additional Bacl2 is added in excess to precipitate the sulphate out.

4. A filter paper of constant weight and cooled in a desicator was weighed and its mass noted.
The precipitated BaSO4 was filtered using the weighed filter paper and drained in a suction
pump.
The filter paper and the residue (BaSO4) were dried and weighed.
CALCULATION
Mass of filter paper=1.048g
Mass of precipitate and fitter paper=3.685g
Mass of precipitate BaSO4 is =3.685-1.048=2.637g
Weight of SO2-4= weight of BaSO4 × gravimetric factor
= weight of BaSO4 × a( gram formula weight of SO2-4)
b( gram formula weight of BaSO4)
BaSO4
Ba2+(aq) + SO2-4(aq)
thus a=1 and b=1
hence weight of SO2-4= 2.637 × [32.066+4(16)]/[137.33+32.066+4(16)]
weight of SO2-4= 2.637×96.066/233.396
= 2.637×0.4116
2weight of SO 4= 1.0853892g
= 1085.3892mg
Mg/L SO4= mgBaSO4 x 411.6
ml sample
= 2.637x10-3 x 411.6
250 x 10-3
=4.342 mg/l
DISCUSSION
The solution was digested to break the bonds in the unknown sample in order to make the
sulphate in the solution free to precipitate with the BaCl2 to form BaSO4. The completeness of
the precipitate is check by adding BaCl2 to the clear solution on the surface of the precipitate if

5. no cloudiness is not form then it indicate that there is no sulphate left out in the solution. Either
wise excess BaCl2 must be added to precipitate the sulphate.
The Barium sulphate precipitate was washed with warm distilled water to free the Cl- ion in the
precipitate. The precipitate freeness of Cl- ion is tested by performing qualitative test of Cl. This
is done by 1ml of 0.1M HNO3 into the filtrate collected during the washing and drops of Ag NO3
is added in drop wise, if AgCl precipitate is formed then it indicates that the Barium sulphate
precipitate needs further washing . if not the then precipitate and the filter paper is dried and
weighed it mass noted as 3.685g
HCl was added to the sample solution to prevent the precipitation of barium salts of weak
PRECAUTION
1. The precipitate was digested to increase the average particle size and reduce coprecipitation.
2. BaCl2 was added slowly amidst effective stirring to reduce relative supersaturation.
3. Completeness of the precipitation was tested for after each digestion by adding drops of
BaCl2.
4. The container that contained BaSO4 was washed with warm water to remove the Cl- salt
present.
5. The filter paper and the precipitate were well dried to ensure accurate weight
measurement.
6. The experiment was carried out at a near boiling point temperature to increase the
solubility of the precipitate at equilibrium and reduce relative supersaturation.
CONCLUSION
It can be deduced that the aims of the experiment were met out as expected. The mass of the
sulphate was 4.342mg/l.
REFERENCE
Analytical Chemistry for Technicians, John Kenkel, 3rd edition, pg 130, 142
Analytical Chemistry Handbook, Pradyot Patnaik, 2nd edition, pg 297
Modern Analytical Chemistry- Harvey, Pg248, 250, 251.
KNUST- Kumasi, Department of Chemistry, Laboratory Manual, Pg 29 & 30.